Vacuum 169 (2019) 108923

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Vacuum
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A modified reference area method to estimate creep behaviour of service- T

exposed Cr5Mo based on spherical indentation creep test
Wenbin Lu, Xiang Ling∗, Sisheng Yang∗∗
Jiangsu Key Laboratory of Process Enhancement and New Energy Equipment Technology, School of Mechanical and Power Engineering, Nanjing Tech University, No. 30 Pu
Zhu South Road, Nanjing, 211816, China

A R T I C LE I N FO A B S T R A C T

Keywords: In this study, indentation creep tests under different conditions were conducted using a self-designed vacuum
Spherical indentation creep test high-temperature indentation creep device to investigate the creep properties of service-exposed Cr5Mo. A
Modified reference area method microstructure test was also conducted and a prominent pile-up was found on the surface of the specimen. We
Creep deformation performed a comprehensive finite element analysis to evaluate the non-uniform deformation characteristics of
Service-exposed Cr5Mo
the spherical indentation creep test. The stress distribution and stress evolution for indenters with different
diameters were also estimated during the test. Subsequently, considering the difficulty of calculating the
equivalent stress owing to the area variation during spherical indentation, a modified reference area method was
proposed. Based on a load relaxation simulation and geometric factor analysis, a general formula for the re-
ference areas of indenters with different diameters was given. Thus, the equivalent stress during spherical in-
dentation could be calculated, and the creep behaviour of service-exposed Cr5Mo was estimated. The results
when using the modified method in this study demonstrated good consistency with the results obtained by the
standard method. To sum up, the spherical indentation creep test has prominent advantages over the uniaxial
tensile creep test in the analysis of in-service components.

1. Introduction critical to establish rational correlations between the properties ob-

It has been a critical issue how to evaluate creep properties of ma-
terials properly, as the structures facing severe operation conditions in
aerospace, nuclear power and petrochemical industries [1]. Generally
speaking, the uniaxial tensile creep test is the standard technique for
estimating the creep behaviour of materials. However, in some situa-
tions, the large size of a specimen restricts the use of the conventional
technique. For instance, the creep performance of in-service furnace
pipes cannot be estimated using this measurement method. The in-
dentation creep test evolved from the conventional indentation test [2]
and was proposed as a technique to evaluate the creep properties of
miniature specimens [3,4]. In addition to its non-destructive nature [5],
the indentation creep test also has the advantage of being able to de-
termine the creep properties of specific materials or materials in loca-
lised regions, such as bulk metallic glasses [6], the heat-affected zone of
welds [7], and so on [8].
To popularise the engineering application of this technique, it is
tained from the indentation creep test and conventional test. Chu et al.
[9] compared the activation energy values obtained from cylindrical
flat indentation and conventional creep tests, and found that the mea-
surements agreed. Based on a conversion factor, Liu et al. [10] pre-
sented a method that set up the relationship between the creep para-
meters of the two tests. However, the contact area continuously rises
when a non-flat indenter is being pressed in by degrees, which makes it
difficult to estimate the creep behaviour. In this regard, a functional
relationship between the contact area and indentation depth for a
Berkovich indenter was established by Brotzen [11], which allowed the
stress at an arbitrary time to be calculated. Besides, a trend of pile-up
normally exists during non-flat indentation, resulting in a complicated
variation of the contact area. Therefore, some researchers have em-
ployed the incremental plasticity theory to revise the contact area
during spherical indentation [12]. Furthermore, Arai et al. [13] pro-
posed a procedure that can estimate the creep exponent and coefficient
from the impression size rather than the penetration depth. Their

∗
Corresponding author. Jiangsu Key Laboratory of Process Enhancement and New Energy Equipment Technology, School of Mechanical and Power Engineering,
Nanjing Tech University, No. 30 Pu Zhu South Road, Nanjing, 211816, China.
∗∗
Corresponding author. Jiangsu Key Laboratory of Process Enhancement and New Energy Equipment Technology, School of Mechanical and Power Engineering,
Nanjing Tech University, No. 30 Pu Zhu South Road, Nanjing, 211816, China.
E-mail addresses: xling@njtech.edu.cn (X. Ling), sishengyang@njtech.edu.cn (S. Yang).

https://doi.org/10.1016/j.vacuum.2019.108923
Received 9 July 2019; Received in revised form 6 August 2019; Accepted 2 September 2019
Available online 04 September 2019
0042-207X/ © 2019 Elsevier Ltd. All rights reserved.
W. Lu, et al. Vacuum 169 (2019) 108923

method avoided the problem of the complicated calculation of the

equivalent stress due to area variation. On the other hand, Takita et al.
[14] proposed a method based on a stress relaxation numerical test,
which made it possible to evaluate the equivalent stress in spite of the
area changing problem. Not only that, various research methods were
used for the instrumentation indentation test, which made the tech-
nique more practical. For example, elastic-plastic cavity expansion
model and slip-line limit method have been developed to analyse the
indentation deformation of plastic materials [15,16]. Ai et al. [17]
proposed a new modified expanding cavity model for characterising the
indentation behaviour of the bulk metallic glass. Besides, inverse
method has also been commonly used for indentation tests [18]. To
systematically estimate the creep behaviours of materials based on
spherical indentation creep tests, it is vital to rationally evaluate the
equivalent stress. However, the pile-up phenomenon and geometric
Fig. 1. Schematic diagram of indentation creep test.
factors during the test make the stress calculation complex. In addition,
the oxidation of the material under high temperature test conditions
may also affect the accuracy of the measurement method. Thus, cor- up with two heating elements. When the thermal expansion was stable,
responding studies ought to be conducted to verify the universality and a constant load was applied to the indenter and transmitted to the
accuracy of the spherical indentation creep test. specimen. By monitoring the creep deformation, indentation depth
In our previous study, another batch of service-exposed materials versus time curves under different loads could be obtained.
were investigated by the small punch creep test [19]. It was proved that
the non-uniform and large deformation did not affect the accuracy of 2.2. Experimental curves and microstructure
the measurement results. Although different service conditions may
lead to changes in material characteristics, it can still be concluded that Typical creep curves for the tensile creep test are shown in Fig. 2.
the creep properties of materials can be reasonably evaluated by micro- Three distinct stages are observed, with the nominal stresses ranging
test technique. Therefore, the indentation creep test is considered in from 160 MPa to 220 MPa. Fig. 3(a) shows spherical indentation depth
present study due to its non-destructive property on specimens. Con- versus time curves, with the applied load ranging from 250 N to 550 N.
sidering the discussion above, this study aims to estimate the creep Similarities and differences exist between the creep curves obtained by
behaviour of service-exposed Cr5Mo on the basis of the spherical in- the two measurement methods. In the primary creep stage, the work
dentation creep test. A vacuum atmosphere was set outside the fixture hardening rate is greater than the recovery rate for creep deformation,
to avoid interference of oxidation. A microstructure test and finite resulting in a decrease in the creep rate with time. Subsequently, the
element analysis were also performed to obtain a rational evaluation of work hardening and recovery rates gradually reach a relatively ba-
the deformation characteristics during the test. Based on the simulation lanced state during the secondary creep stage, which results in a fairly
and geometric factor analysis, a modified reference area method is constant creep rate. For the conventional creep curves, the tertiary
proposed. A general formula for the reference area during spherical stage is observed because of the specimens necking and forming creep
indentation is given, which makes it possible to calculate the equivalent voids [20]. However, no substantial fracture will occur to the specimen
stress at a certain load and time. Finally, the creep behaviour of Cr5Mo in the indentation creep test, and it explains the absence of tertiary
is precisely estimated. We believe that the results of this study would be stage in the creep curves. Compare to other micro-test measurement
meaningful in the analysis of in-service components and further in- methods, a fundamental summary is made. Owing to the destructive
vestigation of the spherical indention creep test. behaviour of specimens in the tertiary creep stage, certain micro-test
measurement results such as small punch creep curves are more similar
2. Experimental to the uniaxial creep curves than the indentation creep curves in the
form of expressions. But the creep characteristics still differ, as the
In order to verify the universality of the indentation creep test, a contribution of the secondary creep time to the overall creep life is
service-exposed Cr5Mo steel sample obtained from a furnace pipe was larger in the micro-test measurement results and the tertiary stage oc-
used in this study. The pipe was in service at 343 °C and 0.26 MPa for cupies the majority of the rupture strain in the uniaxial creep results.
approximately ten years. Considering the maximum service tempera-
ture of the pipes in the same process, all of the following tests were
conducted at 550 °C to obtain a reasonable assessment of the material.

2.1. Experimental procedure

The indentation creep tests were performed using a self-designed

vacuum high-temperature indentation creep device. With a miniature
specimen, the oxidation cannot be neglected because of the tiny creep
deformation. Thus, a vacuum atmosphere was set up to avoid inter-
ference from oxidation to the maximum extent. The fixture structure
and assembly are shown in Fig. 1. A cylindrical flat indenter with the
diameter of 1 mm and spherical indenters with the diameters of 1 mm
and 2 mm were employed in the experiments. Before the test, specimens
were shaped by wire cutting with a size of 10 mm × 10 mm × 3 mm
and then ground with a succession of abrasive paper until using 1200
grit silicon carbide abrasive paper. Thereafter, the furnaces in which the
fixture and specimen were placed on were vacuum pumped and then
heated. To ensure the heating efficiency, the heating apparatus was set Fig. 2. Uniaxial tensile creep curves.

2
W. Lu, et al.
Fig. 3. Experimental curves of indentation creep tests: (a) spherical indenter,
and (b) comparison between cylindrical flat and spherical indenters.
The difference in the form does not affect the accuracy of the analysis.
In contrast, the absence of the tertiary stage in the indentation creep
test makes the deformation more stable and convenient to evaluate.
A comparison between the spherical and cylindrical flat indentation
results is shown in Fig. 3(b). For the flat cylindrical indentation, the
indentation stress is constant during the creep test, and a steady state
can be achieved after a transient primary stage [21]. It is not hard to
understand that the overall stress level of the flat indentation creep is
lower than the spherical one at the same load. Because of the growth of
the contact area, a decrease in the contact stress is inevitable in the
spherical indentation creep test. What we discussed above basically
explains the phenomenon of the spherical indentation creep velocity
being greater than the other one at the same load, but its curve de-
monstrates a more remarkable trend to drop. On the other hand, al-
though the steady-state velocity could not be obtained from the sphe-
rical indentation creep test, the experimental curves still show that the
creep velocity of the spherical indentation tends to be stable by degrees,
similar to the flat one. This indicates that an approximate steady stage
can be achieved in the spherical indentation creep test, because the
growth of the contact area becomes increasingly insignificant after a
sufficiently long creep time. In addition, for both sets of curves, we can
see that the time required to enter the steady stage is gradually
3
Vacuum 169 (2019) 108923
Fig. 4. Optical micrograph of 550 N spherical indentation creep deformation:
(a) overall morphology and (b) local region around indenter.
postponed with an increase in the applied load, and the ratio of the
transient indentation depth to the total indentation depth progressively
increases during the same dwell time.
It is noteworthy that the ideal contact stress should be stable when
the spherical indenter is completely pressed into the specimen, yet the
displacement rate still shows a tiny tendency to change by degrees. We
considered that a trend of pile-up [22] existed on the surface of a
specimen during spherical indentation, resulting in the growth of the
true contact area. Thereby, it brought about the decrease of the
equivalent stress and explained the decrease in the displacement rate.
To verify the theoretical analysis and characterise the creep deforma-
tion, we examined the microstructure under an optical microscope, as
shown in Fig. 4. A prominent pile-up can be seen on the surface of the
specimen, which corresponds to the analysis above. This pile-up phe-
nomenon was also observed in the traditional indentation test. Re-
searchers studied the hardness of materials using the conventional in-
dention test and proposed that the pile-up effect that results in the
deviation of the contact area cannot be ignored [17]. The situation in
this study was very similar because the equivalent stress could not
easily be calculated as a result of the area variation. The following
demonstration could explain the phenomenon to some extent: during
the test, the plastic flow existed and was constrained in a large elastic/
rigid volume in the material. The flow was directed upward and then
appeared as a pile-up on the surface of the specimen [23]. Referring to
the dislocation distribution observed in the vicinity of the indenter and
the creep coefficient mentioned below, the creep deformation me-
chanism of the service-exposed Cr5Mo may be described as dislocation
movement-controlled creep [24]. Besides, two distinguishable regions
could be observed as shown in Fig. 4(b). In the region beneath the in-
denter, the material was found to experience a massive shear de-
formation. The other region, which was not beneath the spherical in-
denter, exhibited no change in the shape of the grains. This revealed the
absence of plastic deformation away from the indentation, showing the
W. Lu, et al. Vacuum 169 (2019) 108923

Fig. 6. Comparison of experimental and simulation curves.

Fig. 5. Finite element model of spherical indentation creep test.

localised nature of the indentation creep deformation [25].

3. Finite element simulation

The aim of the finite element simulation was to further characterise

the creep deformation mechanism of the material. To make a systematic
comparison of the indenter shapes, a spherical indentation creep test
with an indenter diameter of 2 mm was also carried out.

3.1. Finite element model

Based on the symmetrical geometry of the test, a two-dimensional

finite element model was established as shown in Fig. 5. In particular,
the size of the model was consistent with the experiment. The indenter
was set as a rigid body, and the specimen was deformable. The contact
type between the indenter and the specimen was surface-to-surface
contact, and the friction coefficient was set as 0 between them. Based
on fitting using the previously mentioned uniaxial creep curves, B and n
were defined as 3.72 × 10−20 and 7.4, respectively. The plastic para-
meters were described by defining the true plastic strain. The other
theoretical values included a Young's modulus E = 153000 MPa and
Poisson's ratio μ = 0.29. Meanwhile, a similar finite element model
with an indenter diameter of 2 mm was also established for a later
analysis.

3.2. Creep deformation analysis

Fig. 6 shows the indentation depth versus time curves at different

loads for both the experiment and simulation. In general, the simulation
curves display trends similar to those of the experimental curves. It can
be found that the two sets of curves at 300 N almost entirely overlap.
The other simulation curves are slightly lower than the experimental
curves, but they still demonstrate good consistency in the creep stage.
The initial deviation during loading may account for the difference. In
addition, the internal defects of service-exposed materials can also lead
to dispersions of creep results. Therefore, the finite element model es-
tablished in this study was rational.
Fig. 7 shows the evolution of the pile-up on the surface of the Cr5Mo
specimen. We can see that the maximum pile-up on the surface of the Fig. 7. Evolution of pile-up on surface of Cr5Mo specimen: (a) time-dependent
specimen continues to grow with increases in the load and dwell time. and load-dependent evolution with indenter diameter of 1 mm, and (b) time-
For the case where the diameter of the indenter was 1 mm, as shown in dependent evolution at 900 N with indenter diameter of 2 mm.
Fig. 7(a), it was found that when the indenter was gradually pressed in,
the maximum pile-up occurred at a distance of one radius to twice the

4
W. Lu, et al.
Fig. 8. Stress distributions on surface of specimen with dwell time of 30 h: (a) D = 1 mm, F = 450 N; (b) D = 2 mm, F = 900 N.
radius from the symmetric centre. Then, the pile-up decreased with an
increase in the distance and became negligible by degrees after triple
the radius distance. However, the situation was not exactly the same
when the diameter of the indenter was 2 mm, as shown in Fig. 7(b).
Because of the smaller deformation, the indenter was not fully pressed
in. The maximum pile-up occurred at approximately the distance of one
radius from the symmetric centre, and its growth tendency was not as
significant as the former. The pile-up hillocks obtained in the finite
element simulation were somewhat greater than those obtained ex-
perimentally, and similar phenomenon was also observed and illu-
strated by Kucharski [26]. Thus, the accuracy of the finite element
predictions of the pile-up in the vicinity of the indenter could be re-
garded as satisfactory. The size of the pile-up hillock is not quantita-
tively described in this paper, but it is generally believed that the
specific value is related to the strain hardening exponent and the ratio
of yield stress to elastic modulus of the material, and the maximum
indentation depth to the radius of the spherical indenter during the test.
The stress distributions on the specimen surfaces for both cases are
shown in Fig. 8. It is observed that a great stress concentration occurs in
the centre of the contact region and the stress spreads out in the radial
direction from the centre of the specimen. Karthik also studied the
spherical indentation test and concluded that the maximum plastic
5
Vacuum 169 (2019) 108923
strain was at the centre of the contact region and decreased with the
radial distance from the axis of symmetry to the contact edge [27]. This
basically corresponded to the simulation results obtained in this study.
For the latter case, there was a stress concentration at the bulged region
under the contact area of the indenter, which hindered the further
growth of the pile-up. This explained the phenomenon that the evolu-
tion of the pile-up with the indenter diameter of 2 mm had a slower
tendency, as previously mentioned. It was concluded that the largest
strain of the specimen appeared in the necking region by means of
certain micro-test technique in our previous research. However, the
ductile fracture did not occur to the specimen during the indentation
creep test, and the corresponding appearance was a pile-up hillock.
Moreover, the consistency between the finite element analysis results
and microstructure again verified the rationality of the model.
To obtain a more intuitive view of the stress evolution during
spherical indentation, the Mises stress along the axial direction was
extracted separately for the two cases (Fig. 9). In general, with an in-
crease in the creep time, there was a state where the Mises stress gra-
dually decreased as a result of the increase in the contact area. Stress
redistribution with creep time can be observed and the difference in
creep rates during the test is found to be the cause for the phenomenon
[23]. In the former case, we find that the curves in Fig. 9(a) can be
W. Lu, et al.
Fig. 9. Evolution of Mises stress on surface of specimen: (a) D = 1 mm,
F = 450 N; (b) D = 2 mm, F = 900 N.
divided into three regions indicated with Ⅰ, Ⅱ, and Ⅲ respectively. The
first stage shows the trend of slowly decreasing as the contact area
increases by degrees. The second region coincides well with the posi-
tion where the maximum pile-up exists, and the rapid decrease in stress
in this region is due to the plastic flow [28]. For the case with the
indenter diameter of 2 mm, as shown in Fig. 9(b), it can be found that
the maximum stress point occurs slightly before the position of max-
imum pile-up in the radius distance, and there is a significant stress
wave around the bulged region [29]. The following demonstration may
account for the difference of the stress distributions: the indentation
depth has reached a remarkable value in the elastic-plastic stage for the
former case, which is almost half of the radius of the indenter. How-
ever, for the later case, the initial indentation depth is a smaller value
compared with the radius of the indenter. It means that the indenter is
far from fully pressed in, which results in the stress concentration at the
edge of the contact area between the indenter and the specimen and the
obvious stress diversification. Besides, the tertiary stage shows a slowly
decreasing trend once again, and the stress becomes insignificant away
from the indenter, which agrees with the localised nature of the in-
dentation creep deformation.
6
Vacuum 169 (2019) 108923
4. A modified reference area method
It is well known that metallic materials display time-dependent
creep behaviours at high homologous temperatures, and uniaxial creep
tests are generally conducted to determine the relationship between
steady-state strain rate ε̇ c and applied stress σ using the Norton equation
as follows:
ε˙ c = Bσ n (1)
where the constants B and n uniquely characterise this power-law creep
response. Using the uniaxial measurement method, the creep para-
meters can be determined by plotting the measured strain rates against
the applied stresses on logarithmic scales. For the spherical indentation
creep test, the most troublesome problem is that the contact area con-
tinuously changes with the growth of the indentation depth. In addi-
tion, the influence of pile-up, which results in a complicated variation
of the true contact area, cannot be neglected. It has been found that the
reference stress at a certain time cannot be easily calculated. To pre-
cisely estimate the creep behaviour despite the complicated stress di-
versification, a modified reference area method is proposed. We studied
this method using the following procedures on the basis of a load re-
laxation simulation.
In the case of uniaxial loading, the total strain increment is the sum
of the elastic strain increment, plastic strain increment, and creep strain
increment. In the strain maintenance process, the total strain increment
is zero, and the plastic strain remains undeveloped [14]. Taking Hoo-
ke's law into consideration, the creep strain rate ε̇tc can be expressed as
follows：
1
ε˙tc = − σ˙ t
E (2)
where the subscript t denotes a uniaxial condition, E is Young's modulus
and σ̇t is the stress relaxation rate. Using Eq. (2), the creep strain rate ε̇tc
can be calculated from the stress relaxation rate which is obtained as
the slope of the stress relaxation curve.
Because the true contact area increases as result of the pile-up trend
and geometric factor during the spherical indentation, we should give a
rational definition of the reference area, to calculate the corresponding
equivalent stress. The equivalent stress is obtained with the following
procedure using the new reference area Sr . The stress due to the in-
dentation is defined as follows:
F
σt =
Sr (3)
where F is the applied force, and the stress is the value after translating
the multiaxial stress into the tensile stress. In other words, the stress in
Eq. (3) can be regarded as the equivalent stress for the indentation
creep test. Using time differentiation, Eq. (3) is rewritten as follows:
1
σ˙ = F˙
Sr (4)
The load relaxation rate Ḟ in Eq. (4) can be obtained as the slope of
the load relaxation curves which can be derived from the following
finite element analysis. The indentation depth maintenance simulation
used the finite element model established in section 3.1. Ten kinds of
load conditions were employed throughout the process of the spherical
indentation. In the simulation procedure, the indenter was pushed into
the specimen with an equal indentation rate until the predetermined
depth under each load condition. Subsequently, the indentation depths
were kept constant for 2 h, and the load relaxation curves were ob-
tained (Fig. 10).
By substituting Eq. (4) for Eq. (2), the creep strain rate could be
obtained from the load relaxation curve as:
1 ˙
ε˙tc = − F
ESr (5)
Then, using Eq. (3) to calculate the stress for the indentation creep
W. Lu, et al. Vacuum 169 (2019) 108923

Fig. 10. Load relaxation curves during indentation depth maintenance.

Fig. 11. Relationship between reference area and ideal contact area.

test, the following equation can be obtained with Eqs. (1), (3) and (5)
In addition, Eq. (8) can be simplified into Eq. (10):
as:
ni Sc = πh (D − h) (10)
1 ˙ F
− F = Bi ⎛ ⎞
⎜ ⎟

ESr ⎝ Sr ⎠ (6) Eq. (9) can be rewritten as Eq. (11):

where Bi and ni are the creep coefficient and creep exponential obtained Sr = k2 h (D − h) (11)
on the basis of the indentation creep test, respectively. The reference
The diameter D of a particular spherical indenter is a fixed value.
area is defined as the area where the stress is kept constant during the
Numerous researchers have applied indentation creep tests to evaluate
load relaxation. If the stress is obtained in the reference area, Sr , Nor-
the superficial properties of specimens. If the indentation depth h is a
ton's law should give the same values for both the indentation creep test
small value compared to the diameter D, the reference area can be
and uniaxial creep test. Consequently, using the material constants B
linearly fitted as a function of indentation depth h. Choosing the values
and n in Norton's law, the new reference area Sr is expressed as the
until the indenter is half pressed, it is found that the reference area and
following equation:
indentation depth still have a proportional relationship with a small
1 deviation, and the fitting results share a nearly common coefficient as
−F˙ ⎫1 − n
Sr = ⎧ n⎬
before (Fig. 12).
⎨
⎩ BEF ⎭ (7) In some cases such as thick wall in-service pipes, the creep prop-
In other words, the reference area corresponding to an indentation erties of a material may not be accurately evaluated with a small in-
depth can be calculated using Eq. (7). dentation depth. Thus, it is also necessary to obtain a rational evalua-
Meanwhile, another series of numerical analyses with an indenter tion of the creep performance of materials with a large indentation
diameter of 2 mm was also conducted following the same steps. Taking depth, and the corresponding reference area needs to be obtained.
the geometric factor into consideration, there should be a certain re- Based on the fitting results shown in Fig. 13, the modified reference
lationship between the reference area and the ideal contact area. Each area for spherical indentation is defined as follows:
reference area calculated by Eq. (7) and obtained from the specific
relationship with the ideal contact area should have the same value at a
given indentation depth. This implies that we can plot a scatter diagram
of the reference area versus the ideal contact area to verify the re-
lationship between them. For the spherical indenter, the ideal contact
area is calculated by Eq. (8):

Sc = π (r 2 − (r − h)2) (8)

where r is the radius of the indenter and h is the indentation depth. The
scatter diagrams of the reference area versus ideal contact area of cases
with different diameters are shown in Fig. 11. We can see that the re-
ference area is proportional to the ideal contact area, with a small de-
viation. Thus, it can be claimed that during the indentation creep test,
the reference area normally depends on the ideal contact area Sc , as
follows:
Sr = k1 Sc (9)

where k1 is a constant related to the material properties and test con-

ditions. By the substitution of Eqs. (7)–(9), the constant k1 can be ob-
tained, and both the fitting results have similar values. This verifies the
reliability of the linear relationship and proves the versatility of the Fig. 12. Relationship between reference area and indentation depth till in-
method for distinct indenters. denters half pressed.

7
W. Lu, et al.
Fig. 13. Determination of modified reference area: (A) D = 1 mm and (B)
D = 2 mm.
Sr = krh (12)
where k is a constant related to the material properties and test con-
ditions, r is the indenter radius and h is the indentation depth.
Considering the indentation depth versus time curves under dif-
ferent loads are obtained using indentation creep tests, the equivalent
stress at a certain load and time can be calculated. The creep strain rate
for spherical indentation can be evaluated by the following equation
[30]:
h˙
ε˙ c =
h (13)
where ḣ is the displacement rate obtained from the experimental curve.
From now on, we can establish the relationship between the creep
strain rate and equivalent stress at a certain load using Eqs. (1), (3),
(12) and (13). Using the modified reference area presented in
Fig. 13(a), we can determine the creep parameters by plotting the creep
strain rates against the equivalent stresses on logarithmic scales, and
make a comparison with the conventional measurement (Fig. 14). The
creep constant B and creep exponential n for the spherical indentation
creep test are 9.08 × 10−19 and 7.04, while the values obtained from
the uniaxial creep test are 3.72 × 10−20 and 7.4, respectively. It is
noteworthy that the creep exponentials obtained by both measurement
methods demonstrate good consistency. The creep constant remains
some deviations, but within a reasonable range. Considering the
8
Vacuum 169 (2019) 108923
Fig. 14. Comparison of relationship between stress and creep strain rate.
particularity of the service-exposed material investigated in this study,
it should be noted that more experimental tests for other materials and
more in depth physical characterisation and more accurate physically
based numerical modelling are needed in order to further evaluate the
feasibility of the modified reference area method before putting it to
practical application.
Conclusively, by applying the previously discussed procedures, it
was possible to obtain the creep parameters of the service-exposed
Cr5Mo, which corresponded to the fitted value from the conventional
method. Because the indentation creep test is a miniature test, it can
effectively and economically evaluate creep properties of in-service
components. However, the problem of the complicated stress calcula-
tion restricts the engineering application of the spherical indention
creep test in related fields. Therefore, we believe that the modified
reference area method reported in this paper can provide new insights
for the study of the spherical indentation creep test.
5. Conclusions
This paper aims to estimate the creep behaviour of service-exposed
Cr5Mo and evaluate its creep properties using a modified reference area
method. Above all, indentation and uniaxial creep tests were conducted
under different conditions. Subsequently, finite element simulations
and a series of theoretical analyses were carried out to obtain reason-
able evaluations of the material. The main conclusions are as follows:
(1). Experiments with the service-exposed Cr5Mo under different con-
ditions were conducted. The results showed that the creep per-
formance of the material could be reasonably evaluated using the
spherical indentation creep test.
(2). A microstructure test and finite element analysis were performed
to evaluate the non-uniform deformation characteristics of the
spherical indentation creep test.
(3). An estimation of creep stress during the test was performed. The
stress distributions and stress evolutions of indenters with different
diameters were distinct, accounting for the difference in the evo-
lution of the pile-up.
(4). A modified reference area method was proposed based on the load
relaxation simulation and geometric factor analysis. A simple
linear relationship was established between the reference area and
indentation depth, and the equivalent stresses for distinct indenters
during spherical indentation at arbitrary times could be calculated.
(5). The modified reference area method reported in this paper made it
possible to precisely evaluate the creep exponential of service-ex-
posed Cr5Mo based on the spherical indentation creep test.
W. Lu, et al. Vacuum 169 (2019) 108923

Acknowledgements [15] S.C. Wright, Y. Huang, N.A. Fleck, Deep penetration of polycarbonate by a cy-
lindrical punch, Mech. Mater. 13 (4) (1992) 277–284 https://doi.org/10.1016/
0167-6636(92)90020-E.
This work is supported by National Natural Science Foundation [16] R.T. Shield, On the plastic flow of metals under conditions of axial symmetry, Proc.
Project of China (Grant No. 51805245) and China Postdoctoral Science R. Soc. Lond. 233 (1193) (1955) 267–287 https://doi.org/10.1098/rspa.1955.
Foundation (2017M621738). 0262.
[17] K. Ai, L.H. Dai, A new modified expanding cavity model for characterizing the
spherical indentation behavior of bulk metallic glass with pile-up, Scr. Mater. 56 (9)
References (2007) 761–764 https://doi.org/10.1016/j.scriptamat.2007.01.017.
[18] O. Iracheta, C.J. Bennett, W. Sun, A holistic inverse approach based on a multi-
objective function optimisation model to recover elastic-plastic properties of ma-
[1] Y.B. Hu, L. Zhang, C.Q. Cheng, P.T. Zhao, T.S. Cao, G.P. Guo, J. Zhao, Influence of
terials from the depth-sensing indentation test, J. Mech. Phys. Solids 128 (2019)
specimen thickness on the creep behavior of a directional solidification nickel-based
1–20 https://doi.org/10.1016/j.jmps.2019.04.001.
superalloy, Vacuum 150 (2018) 105–115 https://doi.org/10.1016/j.vacuum.2018.
[19] S.S. Yang, Y.Y. Zheng, Y.J. Duan, X. Ling, Creep characteristics and deformation
01.032.
analysis of service-exposed material using small punch creep test, Eng. Fract. Mech.
[2] A.C. Fischer-Cripps, A review of analysis methods for sub-micron indentation
195 (2018) 242–252 https://doi.org/10.1016/j.engfracmech.2018.04.025.
testing, Vacuum 58 (2000) 569–585 https://doi.org/10.1016/S0042-207X(00)
[20] B.A. Esgandari, B. Nami, M. Shahmiri, A. Abedi, Effect of Mg and semi solid pro-
00377-8.
cessing on microstructure and impression creep properties of A356 alloy, T.
[3] D.H. Sastry, Impression creep technique—an overview, Math. Sci. Eng. 409 (1)
Nonferr. Metal. Soc. 23 (9) (2013) 2518–2523 https://doi.org/10.1016/S1003-
(2005) 67–75 https://doi.org/10.1016/j.msea.2005.05.110.
6326(13)62763-6.
[4] S.N.G. Chu, J.C.M. LI, Impression creep; a new creep test, J. Mater. Sci. 12 (1977)
[21] H. Wang, Q.D. Wang, C.J. Boehlert, J. Yang, D.D. Yin, J. Yuan, et al., The im-
2200–2208 https://doi.org/10.1007/BF00552241.
pression creep behavior and microstructure evolution of cast and cast-then-ex-
[5] B.X. Xu, X.M. Wang, B. Zhao, Z.F. Yue, Study of crystallographic creep parameters
truded Mg–10Gd–3Y–0.5Zr (wt%), Math. Sci. Eng. 649 (2016) 313–324 https://doi.
of nickel-based single crystal superalloys by indentation method, Math. Sci. Eng.
org/10.1016/j.msea.2015.10.001.
478 (2008) 187–194 https://doi.org/10.1016/j.msea.2007.07.038.
[22] R.S. Ginder, W.D. Nix, G.M. Pharr, A simple model for indentation creep, J. Mech.
[6] Y.D. Sun, Z.Q. Li, J.S. Liu, M.Q. Cong, J.Y. Qin, Indentation creep behaviors of
Phys. Solids 112 (2018) 552–562 https://doi.org/10.1016/j.jmps.2018.01.001.
Mg61Cu28Gd11 and (Mg61Cu28Gd11)99.5Sb0.5 bulk metallic glasses at room
[23] J. Naveena, G. Kumar, M.D. Mathew, Finite element analysis of plastic deformation
temperature, J. Rare Earths 29 (2011) 253–258 https://doi.org/10.1016/S1002-
during impression creep, J. Mater. Eng. Perform. 24 (4) (2015) 1741–1753 https://
0721(10)60441-3.
doi.org/10.1007/s11665-014-1225-z.
[7] W. Sun, T.H. Hyde, A potential method for determining the haz properties in welds
[24] M. Kim, K.P. Marimuthu, S. Jung, H. Lee, Contact size-independent method for
using two-material impression creep test, Acta. Metall. Sin-Engl. 17 (4) (2004)
estimation of creep properties with spherical indentation, Comput. Mater. Sci. 113
591–596 http://www.amse.org.cn/EN/Y2004/V17/I4/591.
(2016) 211–220 https://doi.org/10.1016/j.commatsci.2015.11.044.
[8] R. Seltzer, Y.-W. Mai, Depth sensing indentation of linear viscoelastic–plastic solids:
[25] V. Shankar, P. Parameswaran, M.D. Mathew, Impression creep deformation beha-
a simple method to determine creep compliance, Eng. Fract. Mech. 75 (17) (2008)
viour of 316LN stainless steel, Mater. A. T. High. Temp. 32 (6) (2015) 583–591
4852–4862 https://doi.org/10.1016/j.engfracmech.2008.06.012.
https://doi.org/10.1179/1878641315Y.0000000004.
[9] S.N.G. Chu, J.C.M. LI, Impression creep of β-tin single crystals, Math. Sci. Eng. 39
[26] S. Kucharski, S. Stupkiewicz, H. Petryk, Surface pile-up patterns in indentation
(1979) 1–10 https://doi.org/10.1063/1.1722705.
testing of Cu single crystals, Exp. Mech. 54 (6) (2014) 957–969 https://doi.org/10.
[10] Y.J. Liu, B. Zhao, B.X. Xu, Z.F. Yue, Experimental and numerical study of the
1007/s11340-014-9883-1.
method to determine the creep parameters from the indentation creep testing,
[27] V. Karthik, P. Visweswaran, A. Bhushan, D.N. Pawaskar, K.V. Kasiviswanathan,
Math. Sci. Eng. 456 (1–2) (2007) 103–108 https://doi.org/10.1016/j.msea.2006.
T. Jayakumar, et al., Finite element analysis of spherical indentation to study pile-
11.098.
up/sink-in phenomena in steels and experimental validation, Int. J. Mech. Sci. 54
[11] F.R. Brotzen, Mechanical testing of thin films, Int. Mater. Rev. 39 (1) (1994) 24–45
(1) (2012) 74–83 https://doi.org/10.1016/j.ijmecsci.2011.09.009.
https://doi.org/10.1109/SENSOR.1991.149045.
[28] T.S. Byun, J.D. Hunn, K. Farrell, L.K. Mansur, E.H. Lee, Characterization of plastic
[12] H. Lee, J.H. Lee, G.M. Pharr, A numerical approach to spherical indentation tech-
deformation in a disk bend test, J. Nucl. Mater. 294 (3) (2001) 256–266 https://doi.
niques for material property evaluation, J. Mech. Phys. Solids 53 (9) (2005)
org/10.1016/S0022-3115(01)00484-6.
2037–2069 https://doi.org/10.1016/j.jmps.2005.04.007.
[29] H. Toyama, H. Kishida, A. Yonezu, Characterization of fatigue crack growth of
[13] M. Arai, High-temperature creep property of high-Cr ferritic heat-resisting steel
concrete mortar under cyclic indentation loading, Eng. Fail. Anal. 83 (2018)
identified by indentation test, J. Press. Vess-T ASME. 139 (2) (2016)
156–166 https://doi.org/10.1016/j.engfailanal.2017.10.004.
021403https://doi.org/10.1115/1.4033943.
[30] R. Hill, Similarity analysis of creep indentation tests, P. Roy. Soc. 436 (1992)
[14] A. Takita, K. Sasaki, K.-i. Ohguchi, A method to identify steady creep strain from
617–630 https://doi.org/10.1098/rspa.1992.0038.
indentation creep using a new reference area of indentation, J. Electron. Mater. 43
(7) (2014) 2530–2539 https://doi.org/10.1007/s11664-014-3196-0.